Реакция #1951040

ord-0882813f51584fe7be2104a310ff0d3f

Растворители

Условия реакции

Подробные условия
See reaction.notes.procedure_details.

Обработка

  1. 1
    ДругоеThe resultant reaction mixture
  2. 2
    Концентрированиеwas concentrated under reduced pressure
  3. 3
    workup.ADDITIONa mixture of chloroform and methanol (20:1)
  4. 4
    workup.ADDITIONwas added to the resultant residue
  5. 5
    ФильтрацияThe thus-precipitated crystals were filtered
  6. 6
    Другоеthe resultant crystals were recrystallized from water

Методика

Compound 3 (200 mg, 0.53 mmol) was dissolved in methanol (7.00 ml), and 28% aqueous ammonia (5.00 ml) was added to the resultant solution, followed by stirring at room temperature for four hours. The resultant reaction mixture was concentrated under reduced pressure, and a mixture of chloroform and methanol (20:1) was added to the resultant residue. The thus-precipitated crystals were filtered, and then the resultant crystals were recrystallized from water, to thereby yield compound 4 (113 mg, 0.39 mmol, 73.6%).

Источник

DOI: 10.6084/m9.figshare.5104873.v1Патент: US07625877B2uspto-grants-2009_12